Method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials

A technology of konojirimycin and a detection method, which is applied in the field of content detection of Chinese medicinal materials, can solve the problems of cumbersome and complicated process, inaccurate measurement results, long time consumption, etc., and achieves improved reactivity, improved derivatization reaction effect, and shortened derivatization The effect of reaction time

Active Publication Date: 2018-11-16
CHINA RESOURCES SANJIU MEDICAL & PHARMA +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] For this reason, the technical problem to be solved by the present invention is that the process of measuring the content of white tree medicinal material in the prior art is complicated and time-consuming, and too many extraction and separation steps easily lead to inaccurate measurement results, and then provide a fast, accurate, Convenient detection method of white tree medicinal material

Method used

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  • Method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials
  • Method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials
  • Method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials

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experiment example 1

[0038] 1. Methodological investigation on the determination of α-konojirimycin content by pre-column derivatization method

[0039] 1 Instruments and reagents

[0040] Utimate3000 High Performance Liquid Chromatography (Dianne, USA); Freeze Dryer (Shanghai Zhengqiao Scientific Instrument Co., Ltd.); Centrifuge (Shanghai Luxiangyi Centrifuge Instrument Co., Ltd.); Ultrasonic Instrument (Shanghai Kedao Ultrasonic Instrument Co., Ltd.).

[0041] α-Takanojirimycin reference substance (made by the Institute of Materia Medica, Chinese Academy of Medical Sciences), acetonitrile and methanol are chromatographically pure, water is ultrapure water, anhydrous pyridine and benzoyl chloride are ultra-dry grade, and the rest of the reagents are analytically pure.

[0042] 2 Methods and results

[0043] 2.1 Preparation of reference substance solution, test solution and blank sample solution

[0044] 2.1.1 Preparation of reference solution

[0045] Accurately weigh about 3mg of α-konojirim...

Embodiment 1

[0123] Embodiment 1: (do not add enzyme in the extraction process)

[0124] A method for detecting the content of α-konojirimycin in Radix Radix Medicinae comprises the following steps,

[0125] (1) Preparation of reference substance solution: Accurately weigh 5.932mg of α-konojirimycin reference substance, add 1ml of anhydrous pyridine to dissolve it completely, then add 0.3ml of benzoyl chloride and 1.0ml of dichloromethane in turn, seal , react in a water bath at 60°C for 40 minutes, add methanol to the reacted solution to 25ml, accurately measure 2ml, add methanol to 25ml, and make α-konojirimycin reference substance mother solution containing 18.9μg per 1ml, shake well , filtered through a 0.45 μm membrane filter, and the filtrate was obtained;

[0126](2) Preparation of standard curve: Take the reference substance solution prepared in step (1), pipette 0.2ml, 0.5ml, 1.0ml, 2.0ml, 3ml, 5ml into a 10ml volumetric flask precisely, add methanol to dilute to volume, Make a ...

Embodiment 2

[0130] Embodiment 2: (add 0.05g enzyme in the extraction process)

[0131] A method for detecting the content of α-konojirimycin in Radix Radix Medicinae comprises the following steps,

[0132] (1) Preparation of reference substance solution: Accurately weigh 11.861mg of α-konojirimycin reference substance, add 1.5ml of anhydrous pyridine to make it completely dissolved, then add 0.5ml of benzoyl chloride and 1.5ml of chloroform in turn, seal, React in a water bath at 50°C for 40 minutes, add methanol to the reacted solution to 50ml, accurately measure 2ml, add methanol to 25ml, and make a mother solution of α-konojirimycin reference substance containing 18.9μg per 1ml, shake well, Filter through a 0.45 μm filter membrane, and take the subsequent filtrate to obtain the product;

[0133] (2) Preparation of standard curve: Take the reference substance solution prepared in step (1), pipette 0.2ml, 0.5ml, 1.0ml, 2.0ml, 3ml, 5ml into a 10ml volumetric flask precisely, add methanol...

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Abstract

The invention relates to the field of traditional Chinese medicine content detection, in particular to a method for detecting content of alpha-homonojirimycin in suregade glomerulata medicinal materials. According to the method, alpha-homonojirimycin is taken as a control, acyl chloride derivatization reagents are used for precolumn derivatization of alpha-homonojirimycin, dichloromethane or chloroform is added to accelerate the reaction, an AgilentExtendC18 chromatographic column is used as the chromatographic column, and the mixture of methanol, acetonitrile and water is used as the mobile phase, and separating determination and quantitative analysis of alpha-homonojirimycin is conducted with high performance liquid chromatography. The detection method for the suregade glomerulata medicinal materials is quick, accurate and convenient.

Description

technical field [0001] The invention belongs to the field of content detection of traditional Chinese medicinal materials, and in particular relates to a content detection method of α-konojirimycin in white tree medicinal materials. Background technique [0002] α-glucosidase inhibitors are an important class of oral drugs used clinically to treat diabetes. Representative drugs of the existing α-glucosidase inhibitors include acarbose, voglibose, and rice. Glitol. Unlike oral hypoglycemic drugs such as biguanides, insulin sensitizers, and insulin secretagogues, which need to be metabolized by the liver and kidney in the body, which limits the use of patients with abnormal liver and kidney function, α-glucosidase inhibitors can inhibit intestinal epithelial cells. The surface α-glucosidase activity targets the small intestine, which can delay the absorption of carbohydrates without inhibiting the absorption of protein and fat, and has almost no side effects and accumulation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/067G01N2030/8809
Inventor 李琼娅徐冰刘志刚陈周全马鹏岗韩晓强陈若芸王洪庆
Owner CHINA RESOURCES SANJIU MEDICAL & PHARMA
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